Structural investigations on PZT precursors for thin film preparation

Kolb, U.; Abraham, Ingo; Gutwerk, Dieter; Ertel, Teja S.; Hörner, W.; Bertagnolli, Helmut; Merklein, S.; Sporn, D.

doi:10.1016/0921-4526(94)01074-b

Cited by 4 publications

(6 citation statements)

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“…The differences between the results of Ahlfa ¨nger and Payne may reflect real differences in the samples studied as both the chemistry used to prepare the gels and the heat treatments of the samples differed markedly. A later EXAFS study on dry PZT gels, prepared by the same method as Ahlfa ¨nger et al, at the Zr K-and Pb L III -edges was interpreted as indicating that there were probably no Zr-O-Pb links in the samples examined, 19 in apparent contradiction with earlier Raman studies. 20 Recent EXAFS studies of lead titanate gels by Antonioli, et al 21 suggest that Pb-O-Ti links do not occur in these materials.…”

Section: Introductionmentioning

confidence: 65%

“…25,30 However, the refinements for samples PZT-SGH1 and SGH2 clearly demonstrate that our adaptation of a widely used sol-gel route to PZT also produces two-phase samples even after a high-temperature heat treatment. The presence of the two phases is associated with compositional inhomogeneity in the sample and does not require an explanation based on the "quenched in thermal fluctuations" hypothesized by Cao et al 35 While there is strong evidence in the literature that PZT gels and glasses prepared by alkoxide sol-gel chemistry are compositionally inhomogeneous (see the Introduction), 13,17,19,21 reports on the use of solution preparation methods for compositions close to the morphotropic phase boundary usually claim a relatively narrow region for phase coexistence 32,34 and we are not aware of any other work indicating that the rhombohedral component differs so greatly in composition from that of the bulk sample. The large difference between the compositions of the two phases could arise for a number of reasons: (i) the zirconium-rich rhombohedral phase could be a remnant of the compositional inhomogeneity that other workers 7,13,24 have observed in PZT glasses prior to complete crystallization, (ii) the rapid heating used for samples PZT-SGH1 and SGH2 could have led to compositional segregation during the firing process, or (iii) there may be a miscibility gap in the phase diagram.…”

Section: Discussionmentioning

confidence: 99%

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Neutron Scattering Studies of Compositional Heterogeneity in Sol−Gel Processed Lead Zirconate Titanates

Wilkinson

Pattanaik

et al. 1998

Chem. Mater.

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Rietveld analyses of neutron diffraction data collected on a series of Pb(Zr 0.5 Ti 0.5 )O 3 samples, which had been prepared by sol-gel and conventional mixed oxide methods, showed that each sample contained both rhombohedral and tetragonal PZT (Pb[Zr 1-x Ti x ]O 3 ). The zirconium-to-titanium ratio in the two phases was found to be markedly different. Pair distribution functions were also calculated for some of the samples. The inability of a commonly used alkoxide-based sol-gel processing method to produce compositionally homogeneous samples is attributed to a compositional segregation that occurs early on during sol-gel processing and is not fully eliminated on high temperature heat treatment of the samples. A deliberate attempt to produce compositionally inhomogeneous materials, via the separate prehydrolysis of lead titanate and lead zirconate precursors, followed by mixing the resulting sols, was found to induce no more inhomogeneity than is present in materials prepared via the hydrolysis of precursors that were completely mixed.

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Section: Introductionmentioning

confidence: 65%

Section: Discussionmentioning

confidence: 99%

Neutron Scattering Studies of Compositional Heterogeneity in Sol−Gel Processed Lead Zirconate Titanates

Wilkinson

Pattanaik

et al. 1998

Chem. Mater.

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“…This work is an extension of our experiments on other solution-processed zirconium-and titaniumcontaining ceramics. 19 There have been several X-ray absorption spectroscopy (XAS) studies of the local structures around zirconium and titanium in solution-processed high dielectric constant materials such as PZT [20][21][22][23][24][25][26][27][28] and calcium zirconium titanate (CZT). 19 However, there has been very little work on pure zirconium titanates.…”

Section: Introductionmentioning

confidence: 99%

“…There have been several X-ray absorption spectroscopy (XAS) studies of the local structures around zirconium and titanium in solution-processed high dielectric constant materials such as PZT − and calcium zirconium titanate (CZT) . However, there has been very little work on pure zirconium titanates.…”

Section: Introductionmentioning

confidence: 99%

X-ray Diffraction and X-ray Absorption Spectroscopy Studies of Sol−Gel-Processed Zirconium Titanates

Lind

Wilkinson

et al. 2000

Chem. Mater.

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ZrTiO 4 samples were prepared by using a conventional hydrolytic alkoxide sol-gel route, a nonhydrolytic method, an acetic acid modified route, and by the direct reaction of the binary oxides. The local structure in the gels and its evolution upon heating was followed using EXAFS and XANES, and the crystallization of the products was examined using powder X-ray diffraction. All the solution-processed materials crystallized in the range 600-700 °C. The crystalline materials formed at 700 °C showed no evidence of any long-range cation ordering. The EXAFS data indicated that all the amorphous ZrTiO 4 samples produced using the solution routes contained zirconium with a coordination number >6 and that the disordered crystalline ZrTiO 4 contained six-coordinate zirconium. Both the XANES and EXAFS data showed that nearly all the amorphous ZrTiO 4 samples contained titanium with a coordination number of <6. The EXAFS data clearly indicated the presence of Zr-O-Ti links in the ZrTiO 4 gel produced using the nonhydrolytic route. There was also some evidence that the gel prepared using hydrolytic sol-gel chemistry contained Zr-O-Ti links.

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“…Kolb et al 18 used EXAFS to study the local structure of Pb and Zr atoms in liquid and dried amorphous lead zirconium titanium gels prepared by two synthetic methods. The local structure around lead atoms depends on the synthesis conditions in the sol, but the difference disappears after drying.…”

Section: Introductionmentioning

confidence: 99%

A structural study of amorphous alkoxide-derived lead titanium complexes

et al. 1997

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We studied amorphous lead titanium alkoxide-derived heterometallic complexes, prepared from lead acetate and titanium n-propoxide or n-butoxide in parent alcohol medium. According to gas-liquid chromatography (GLC) and thermogravimetric analysis with mass spectrometry of evolved species (TGA/EGA) analyses, the type of alkoxide group influences oxo or acetate bridging, as well as the amounts of hydroxyl and organic groups bound to the metal network. From XANES and EXAFS analysis, local environments of lead and titanium atoms were determined within the analyzed range of 3.4Å. Local environments depend weakly on the type of alkoxide used. Titanium atoms are pentacoordinated. A Pb-Ti correlation is established with lead atoms bound to titanium atoms by oxygen linkages.

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Structural investigations on PZT precursors for thin film preparation

Cited by 4 publications

References 1 publication

Neutron Scattering Studies of Compositional Heterogeneity in Sol−Gel Processed Lead Zirconate Titanates

Neutron Scattering Studies of Compositional Heterogeneity in Sol−Gel Processed Lead Zirconate Titanates

X-ray Diffraction and X-ray Absorption Spectroscopy Studies of Sol−Gel-Processed Zirconium Titanates

A structural study of amorphous alkoxide-derived lead titanium complexes

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